HRID1092863
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Into 1,4-dioxane (1 ml) solution of tetra-n-butylammonium borohydride (638 mg) was added dropwise 1,4-dioxane (1 ml) solution of 2,5-dibromo-4-nitroimidazole (89.5 mg) at a room temperature, after being refluxed the reaction mixture for 23 hours, excessive reagents were quenched by adding concentrated hydrochloric acid, then water and ethyl acetate were added. The organic layer was washed with an aqueous solution being saturated with sodium chloride, then dried over anhydrous sodium sulfate, and purified by a thin layer chromatography (developing agent: ethyl acetate) to obtain 2-bromo-4-nitroimidazole (44.9 g, yield: 71%) of white powdery product.
WORKUP
后处理
- temperatureafter being refluxed the reaction mixture for 23 hours
- customexcessive reagents were quenched
- additionby adding concentrated hydrochloric acid
- additionwater and ethyl acetate were added
- washThe organic layer was washed with an aqueous solution
- dry with materialdried over anhydrous sodium sulfate
- custompurified by a thin layer chromatography (developing agent: ethyl acetate)